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A method for removing residual solvent in fullerene solids

A residual solvent and fullerene technology, applied in the field of fullerenes, can solve the problems of unsuitable fullerene impurity removal process, fullerene high temperature denaturation solubility, fullerene safety risk, etc. Faster drying rate, easy to scale up effect

Active Publication Date: 2020-12-29
苏州仁生泽发生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the extraction and purification of fullerenes requires the use of a large amount of organic solvents such as toluene and o-xylene. These solvents have a similar conjugated structure to the fullerene carbon cage, so they are very easy to remain in the fullerene material
Residual organic solvents will pose a huge safety risk to the biomedical application of fullerenes, and minimizing the amount of residual solvents in fullerenes has become a key technical problem to be solved urgently
The traditional method is to remove the residual solvent in fullerene by high-temperature vacuum drying, but heating fullerene at high temperature for a long time may easily cause high-temperature denaturation and solubility drop of fullerene, and the drying efficiency is low, which is not suitable for industrialization Fullerene impurity removal process

Method used

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  • A method for removing residual solvent in fullerene solids
  • A method for removing residual solvent in fullerene solids
  • A method for removing residual solvent in fullerene solids

Examples

Experimental program
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Embodiment 1

[0033] Embodiment 1: supercritical carbon dioxide removes fullerene C 60 and C 70 Residual o-xylene in:

[0034] (1) Supercritical drying: take 10g of fullerene C with residual o-xylene solvent respectively 60 and C 70 For solid samples, put them into two sample boats (0.5L, cylindrical), seal the upper and lower ends of the sample boats with a 500-mesh stainless steel filter, put the sample boats into a drying kettle with a heating jacket, and tighten the kettle Cover, insert the temperature measuring platinum resistance; start the cold water circulation pump to pre-cool the booster pump, set the cooling temperature to 5°C, and set the temperature of the drying kettle to 50°C; slowly open the liquid carbon dioxide gas supply valve until the pressure in the drying kettle After it is stable (5MPa), fully open the air supply valve; adjust the flow rate of the booster pump of the frequency converter to about 5L / h (the pump frequency is 20Hz at this time), and stabilize the pre...

Embodiment 2

[0046] Embodiment 2 supercritical carbon dioxide removes fullerene C 60 and C 70 Residual toluene in:

[0047] (1) Supercritical drying: Weigh the fullerene C of 10g residual toluene solvent respectively 60 and C 70 For solid samples, put them into two sample boats (0.5L, cylindrical), seal the upper and lower ends of the sample boats with a 500-mesh stainless steel filter, put the sample boats into a drying kettle with a heating jacket, and tighten the kettle Cover, insert the temperature measuring platinum resistance; start the cold water circulation pump to pre-cool the booster pump, set the cooling temperature to 5°C, and set the temperature of the drying kettle to 50°C; slowly open the liquid carbon dioxide gas supply valve until the pressure in the drying kettle After it is stable (5MPa), fully open the air supply valve; adjust the flow rate of the booster pump of the frequency converter to about 5L / h (the pump frequency is 20Hz at this time), and stabilize the pressu...

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Abstract

The embodiment of the invention relates to a method for removing residual solvents in fullerene solids. The method comprises the following steps that fullerene solids with residual organic solvents are placed in supercutical fluid to be dried, organic solvents left in fullerene can be reduced to be blow the standards of the pharmaceutical industry, and meanwhile the fullerene purity cannot be influenced in the drying process. The method is simple in operation, high in feasibility, efficient, rapid and suitable for preparing high-purity fullerene on a large scale.

Description

technical field [0001] The invention relates to the field of fullerenes, and further relates to a method for removing residual solvents in fullerene solids. Background technique [0002] Fullerene is an atomic cluster with a closed structure composed of different numbers of carbon atoms. It has a unique molecular structure and physical and chemical properties. It has shown important applications in biomedical fields such as tumor treatment, radiation and chemotherapy protection, anti-oxidative damage, and health care. prospect. [0003] The pharmaceutical industry has extremely strict requirements on the impurity content in raw materials, among which solvent residue is a type of impurity that needs to be paid attention to. At present, the extraction and purification of fullerenes requires the use of a large amount of organic solvents such as toluene and o-xylene. These solvents have a similar conjugated structure to the fullerene carbon cage, so they are very easy to remain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): F26B3/04F26B3/34F26B25/00
CPCF26B3/04F26B3/343F26B25/00
Inventor 王春儒李杰武万里牛琦峰
Owner 苏州仁生泽发生物科技有限公司